Réaction #66628

Équation de réaction

2-amino-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-3H-pyrimidin-4-one

phosphorus oxychloride

→

4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine

Rendement 88.0%

Conditions de réaction

Traitement

1. 1
   AutreSolvent was removed under reduced pressure and ice water
2. 2
   workup.ADDITIONwas added
3. 3
   Extractionextracted with methylene chloride
4. 4
   LavageThe organic phase was washed with brine
5. 5
   Séchagedried over anhydrous sodium sulfate
6. 6
   AutreAfter removal
7. 7
   Autreof drying agent
8. 8
   Concentrationthe organic solution was concentrated under reduced pressure

Mode opératoire

A mixture of 2-amino-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-3H-pyrimidin-4-one in phosphorus oxychloride (5 ml) was heated at 110° C. for 40 minutes and stirred at room temperature over night. Solvent was removed under reduced pressure and ice water was added. The aqueous solution was basified with potassium carbonate to pH 9, and extracted with methylene chloride. The organic phase was washed with brine and dried over anhydrous sodium sulfate. After removal of drying agent, the organic solution was concentrated under reduced pressure to yield 4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine as yellow solid (0.043 g, 88%). MS M+H=308.

Source